Process for separating volatile substances



1,622 126 March 22,1927. D E. WECKER PROCESS FOR SEPARATING VOLATILE SUBSTANCES Filed March 13. 1924 2 shee tssheet 1 [/wsf h ec/feh March 22, 1927. 1,622,126

E. WECKER PROCESS FOR SEPARATING VOLATILE SUBSTANCES Filed March 13, 1924 2 Sheets-Sheet 2 Patented Mar. 22, 1927. 1,622,126-

UNITED STATES: PATENT orrlce.

miner wncxnn, or nnrnnnomr, (mum. rnocess roe sarm'rme vonarrm suns'rmcns. Application ma mm 1a, 1924, Serial No. 609,187, and in Germany is. so, 1023.

The present invention is directed. to a liquids into the heated oil.-'. This may be recess for separating volatile substances done, for instance, by using a neutral gas rom less volatile substances. This lnvenfor blowing these liquids into the heated tion is more particularly directed to a procoil. Among the neutral gases which may be a ess for separating fatty acids from soaps employed are carbon dioxide, nitrogen, mixto and from soap-stock and also from oils such tures thereof, superheated steam or dry as whale oils, edible oils and fats. This saturated steam. These gases act as trans process is also directed to the separation of porting or carr ing agents for the above resin oils from resins and also for the sepamentioned liqui s. The oil is heated in the no ration of volatile substances from llgnite neighborhood of 250 to 280 0,, or if the as and coal gas tarsand from petroleum and fatty acids are easily volatilized the oil or like materials. fat may be heated to a lower temperature, It has been previously suggested to treat for instance, about 220 to 250 C; It has neutral fats at a high temperature with inbeen found that the process is materially Ra diiderent and permanent gases for the pur-- aided if the oil is maintained at those temre pose of removing fatty acids'present 1n the per'atures under reduced pressure and the V fats. Hydro n has been most used for this mist of the liquids above mentioned are purpose. I ese gases have been passed blown into this heated oil under such rethrough the fats at such a rate and at such duced pressure. p w a tem erature that the fatty acids are re-' The small liquid particles which are init mov without the use of a vacuum. It has jected in the form of this fine mist on enterbeen proposed to pass superheated steam mg mto the heated oil expand violently and through dehydrated fatty substances under instantaneously and are thus explosively reduced pressure for the same urpose. By yaporized. The heated oil acts as a vaporusing a vacuum, the distillation temperalzer and also as a superheater. This init ture of the'fatty acids was claimed to be stantaneous vaporization is aided by the lowered to about 90 to 150 C. The ind1fvacuum imposed upon the oil. as a result ferent gases, 'such as hydrogen and steam of this violent and explosive evaporation of above mentioned, which are employed in the the injected liquid, within the body of the o ess just described are those which do not oil, an instantaneous expulsion and (llstlllib 8K have a detrimental efi'ect on the material tiou oi. the fatty acids in the oil is effected. treated. Ordinary .steam at 100 G. may be The latter goes over as a thick fog. The employed in the place of superheated'steam, temperature of this dog is lower than the if the fat to be treated is heated to suificienttemperature of the heated oil. If the temly high temperature. peratures are those mentioned previously, 90 An important disadvantage of the recess the temperature of this fog may be in the just described arises from the fact tiat the neighborhood of 120 to 150 C. The action length of time necessary to complete the reabove described is improved and accelerated moval of the fatty acids is very large, Anby using as high a vacuum as possible, for 0 other disadvantagearises from the fact that instance, 30 to 40 m. m. mercury pressure.- 95 in order to remove the last traces of fatty In addition to the removal of the fatty acids a'considerable loss of neutral fat reacids, ill-smelling constituents of the fats sults. Decomposition and polymerization are also removed by this distillation. As a also occurs with-the consequent darkening of result, a complete deodorization of the oil the color of the fat and a deterioration of or fats-is obtained. For instance, in treat- 1 its quality. The above disadvantages are ing cocoanut oil all of the evil smelling avoided by the process descnbed and claimed ketones are also removed with the fatty in this specification. Fatty acids are subacids. It is therefore not necessary to stantially completely removed from oils specially treat the oil to deodorize the same. containing the same without iIIJIIIlOUS efi'ects This process is also applicable to the de- 105 on the fat. .The process comprises the modorization of oils and fats which have been troduction of liquids such as water, benzol, previously freed of fatty acid by well known toluol, and alcohol, in the form of a fine methods, for instance, by treatment with mist into the heated fat or oil. This introalkali.

duction may be effected by blowing the The oils and fats treated by the process of Ill) this invention show no deleterious effects. The color is not spoiled. They do not show any symptoms of polymerization. There is no decomposition; no trace of acroleine being noticeable. The present process in contradistinction to the processes heretofore available, is capable of treating oils with a larger variation of fatty acid content. Thus oils varying from about 5% to .or more of free fatty acids may be treated with a substantially complete removal of fatty acid and the complete deodorization. The acid content of the oil treated by thisprocess is from 0.3% to 0.1%, that is a substantially quantitative deacidification has been affected. This deacidification by the injection of liquids, such as water, is surprising in view of the fact that the heatingof neutral fats and water for the purpose of hydrolyzing the oils is well known. The effect of finely distributed water preferably in conjunction with the application of vacuum on highly treated oils is therefore surprising.

As was said previously, the liquids which are to be injected may be carried by gases which have no detrimental efiects on the substances to be treated. Such gases, as was pre viously stated, may be carbon dioxide or nitrogen, mixtures thereof, such as flue gases from which the oxygen has been removed, and hydrogen. Superheated steam may be employed as a carrier for the atomized liquids. When using water as the injected liquid saturated or even superheated steam may be employed. This steam is charged with moisture to convert it into a wet steam. WVet steam directly produced may also be employed for this purpose. The temperature of the steam should be preferably at 100 to 180 C. and under a corresponding pressure.

The following examples are given as illustrative of this invention.

1.Two kilograms of Arachis oil contain-- in about 13% of fatty acids are heated to 280 C.in an. autoclave or in a series of autoclaves. A vacuum corresponding to 30 m. m.

caught in a condenser.

mercury column is toclave. A heated current of carbon dioxide carrying a mist of water suspended therein is injected into the heated oil by means of a suitably constructed nozzle. If a series of autoclaves is employed a separate nozzle is provided for each container. The fatty acid vapors which escape as the thick fog are After treating for five to eight minutes the oil contains only 0.2% free fatty acids.

2.-Cocoanut oil containing 1% of free fatty acids is heated according to the method described under Example 1 to about 250 C. \Vater at a ten'iperature of 100 C. is sprayed into superheated steam at a temperature of 150 C. and at a pressureof'2 atm. The mixture is immediately injected into the .maintained upon the an heated oil. complete after about three minutes treatment. The oil, after treatment, contains about 0.1% free fatty acids.

3.Sesame oil containing about 5% free fatt acid is treated by the method of Examp e 1. The oil is heated to about 270 C.

Wet steam at about 130 C. is injected into The deacidificationof the oil is.

the oil for about 8 to 10 minutes. The wet steam which is injected may be wet steam directl formed or formed by mlxlng ordinary dry ive steam with water. After this treatlnent of the oil it contains about 0.3% fatty acids. a

In carryingout the processes above described, it is advantageous to employ-series connected vessels. The oil or fats are introduced into the vessel'at one end of the series and caused to flow at a .regulated rate through the vessels. This rate is so regulated that the oil on exiting from the series will have been treated for the desired time. The rcactionvessels are advantageously provided with distributing devices to insure a thorough mixing of the injected liquid spray and the substance to be treated. This can be obtained by employing baflles orfilling bodies such as Rasehig-rings and also by subdi- .-viding the reaction vessels into intercomof reaction vessels connected in series, the

first three vessels from the left being shown in elevation, the two last in longitudinal section.

Fig. 2 shows on a larger scale a cross sec- 'tion through a reaction vessel and the conduits connected thereto. I

' Fig. 3 shows an apparatus with a reaction vessel in tower form, in which the substances to be treated and the atomized liquid are led in countercurrent to one another.

In Fig. 1 the various reaction vessels have been indicated by a they are connected with one another by conduits b. The oil or fat is preferably admitted near the bottom of the vessels by means of purified substances leaving which are preferably cooled when flowing off through the conduit (1, collect in the con tainer e. The containers is preferablyconneeted to a vacuum by means of the conduit f.

The expelled volatile substances, for example the fatty acids are removed through the conduit 9 and after they have preferably passed through a cooler it they pass into the collectdr 2' which is also connected to a high vacuum diar duit k.

The finely distributed liquids, for instance the mixture of gas and atomized liquid are admitted through the intermeof the conduit Z, from which branch con uits m lead into the lower part of each vessel a. At the lower end of the conduit m are provided one or more annular connections, which are provided with noz zles or fine openings 0 for the outlet-of the atomized liquid.

Fig. 2 shows on a somewhatlarger scale a section of a vessel a with the outlet pipe g connected to the upper part of the vessel, for the fatty acids, as well as with the admission conduit for the liquid .vapor 1 and the branch conduits m and n with the nozzles 0.

The apparatus shown in Fig. 3 consists of for instance by means of the conthe tower-lilre reaction vessel a, preferably arran ed vertically or slightly'inclined and provided with distributing members or'filling members for instance Rasch1g rm s.

The raw material, for instance the at or oil enters through the conduit d leading into the upper part of the reaction tower a", preferably in an extension c of the same.

During the treatment, the 011 or fat flows through the reaction vessel a in a downward direction and at the lower end of the vessel passes into an extended collecting space c from which it flows through the cooler f to the collector g. The latter is connected with the vacuum for instance through the conduit it.

The volatile substances escaping during the reaction, for instance the fatty acids, are led through the conduit z" to the cooler is and thereupon pass into the collector Z. The latter is connected with a high vacuum by means of the conduit m.

The finely distributed liquids or mixturesor gas andatomized liquid are admitted in the lower part of the reaction tower a by means or the conduit n. liquids entering through these upwards in countercurrent to owing downwards. The reaction vessel It can be heated for instance bymeans ofa heating jacket 0, for instance by a connection with a hot air pipe. (gr steam pipe by means of the conduits an a p Anot er important advantage of this process resides the substances in the fact that certain constituents which are not removed by distillation are precipitated. For example, the such as sesame oil, or Arachis'oil, is greatly improved and becomes much lighter. Asa result of the treatment above described the color matter which is present in colloidal solution,. for example, chlorophyll, phlobaphene is broken'up and hydrolyzed move the fatty acids from The atomized conduits move "mist, said liquid being highly volatile temperature to which the precipitated. The reci itation of these colloids is accelerate an presence of substances which will coagulate at the temperatures. employed. For instance, albuminoids which are always resent in the crude oils are coagulated by t e tempera ure employed and cause 'a precipitation of the colloids; Most likely albuminoid, on flhcculating, occludes the col-' oring matter and therefdre clears up the oil by t e removal of these colloids. I

The present process finds an important application in the manufacture of soap, oleine and stearine. It is usual in this industry to hydrolyze the fats to form glycerineand fatty acids. The glycerine is then separated by washing, leaving a mixture of about 85% fatty acids and about 15% unneutral fats. This. mixture is then subjected to ordinary distillation to rethe neutral tats. During this distillation a acids and es eciallyneutral tat undergoes pyrogenous ecomposition. In consequence, so called stearine pitch, acroleine and other byproducts and residues are obtained.

he above disadvantages ma be avoided by employing the process of t is invention for the separation of the fatt acids from the neutral fats. The hydrolysis may-be carried out to a smaller degree than" is usual, for instance, to obtain about free fatty acids. The mixture of free fatty acids and neutral fats obtained utter the removal of the glycerine may be treated by the process above described. The residual neutral late after removal of free fatty returned for further hydrolysis.

lin the following claims by the term oils I mean to include oily substances, commonly known as oils and tats.

The above description is to be taken not as limiting my invention, but merely illustrative of LA process of refining oil containing fatty aci swhich comprises heating said oils to an elevated temperature, in'ecting into said oils a liquid in the form 0 a fine at the I oil has been heated, thereby producing an-insta'ntaneous expansion and volatilization of the injected liquid and vaporizing the fatty acids in the oil and withdrawing said vapor.

2. The process of refining oil containing fatty acids which comprises heating said oils to an elevated temperature, injecting into said oils a liquid in the form of a fine mist suspended in a neutral carrier gas, said liquid bein highly volatile at the temperature to w ich the oil -has been heated,

thereby producing an instantaneous expanincreased by the the coagulated part of the fatty acids may be the. invention, which ll claim to be:

3. 1 rocessof refining oils containin which the oil has been heated, thereb profatty acids which COIHPIISGS' heatin sai .ducing an instantaneous expansion angvolaoils to an elevated temperature an in a tilizatlo'n of the injected hquid and vapor- 10 vacuum, ine'cting'in sand oils a liquid hf izing the fatty acids in the oil and withdrawthe form 0 a fine mist suspended in a neuing said va por.

tral carrier gas, said liquid being highly In testimony whereofI affix my signature. -volatile at the'temperature and pressureto ERNST WECKER. 

